PREPARATION OF DICYCLOHEXYLCARBODIIMIDE

    公开(公告)号:JPS60166653A

    公开(公告)日:1985-08-29

    申请号:JP1986784

    申请日:1984-02-08

    Abstract: PURPOSE:To obtain economically the titled compound of high quality useful as a dehydration condensing agent in synthesizing peptides, nucleic acid, etc., oxidation reaction assistant, etc., by treating dicyclohexylurea wit phosphorus oxychloride, and treating the resultant product without contact with water. CONSTITUTION:Dicyclohexylurea is reacted with an almost equimolar amount of phosphorus oxychloride in the presence of a pyridine base in large excess at 70-110 deg.C for 1-5hr. The resultant reaction product solution is then heated to

    PRODUCTION OF BENZONITRILE COMPOUND

    公开(公告)号:JPS6032758A

    公开(公告)日:1985-02-19

    申请号:JP13763683

    申请日:1983-07-29

    Abstract: PURPOSE:To produce the titled compound useful as a raw material of pharmaceuticals, agricultural chemicals, etc., in high yield and purity, by reacting a benzoic acid compound with urea in molten state keeping the reaction mixture to a temperature above a specific temperature at least in the latter stage of the reaction. CONSTITUTION:The objective benzonitrile compound is obtained by reacting a benzoic acid compound with urea in molten state keeping the reaction mixture at a temperature above a specific temperature at least in the latter stage of the reaction. In the former stage of the reaction, the benzoic acid compound is made to react with urea to form mainly a benzamide compound, and when the benzoic acid compound is converted almost completely to the benzamide compound, the reaction mixture is heated at >=220 deg.C in the latter stage of the reaction to convert the benzamide compound to benzonitrile compound. Since the boiling point of benzonitrile compound is usually 220-260 deg.C, the reaction is carried out while distilling out the produced benzonitrile compound from the reactor together with by-produced water. The equilibrium of the reaction is shifted to the product side, and the product can be separated by this process without thermal degradation.

    PREPARATION OF P-CHLOROBENZOIC ACID

    公开(公告)号:JPS5832843A

    公开(公告)日:1983-02-25

    申请号:JP12873081

    申请日:1981-08-19

    Abstract: PURPOSE:To obtain the titled substance having excellent purity and color tone, at high rate of reaction, without producing by-products, by oxidizing p-chlorotoluene at a specific temperature in the presence of a specific amount of acetic acid using a catalyst composed of Co and Br. CONSTITUTION:The titled substance is prepared by oxidizing p-chlorotoluene with O2-containing gas (e.g. air) in 1-5pts.wt. of acetic acid solvent based on 1pt. of p-chlorotoluene, using a catalyst composed of Co (0.02-0.7wt% of acetic acid) and Br (1-10pts.wt. per 1pt. of Co), at 110-200 deg.C. The Co compound is those soluble in the reaction product and free of the counter ions inhibiting the reaction, e.g. bromide, hydroxide, carbonate, aromatic carboxylic acid salt, etc., and the bromine compound is bromine, HBr, bromoacetic acid etc. USE:Raw material of pesticides, pharmaceuticals, dyes, resins, etc.

    PREPARATION OF M-NITROBENZOIC ACID
    24.
    发明专利

    公开(公告)号:JPS5821650A

    公开(公告)日:1983-02-08

    申请号:JP11842581

    申请日:1981-07-30

    Abstract: PURPOSE:To prepare the titled compound useful as a raw material of pharmaceuticals, etc., in high catalytic activity, economically, without causing the combustion decomposition of the reaction product, by oxidizing m-nitrotoluene with an O2-containing gas in a specific amount of acetic acid solvent in the presence of a catalyst system having a specific composition, at a specific temperature. CONSTITUTION:m-Nitrobenzoic acid is obtained by oxidizing m-nitrotoluene with an O2-containing gas in acetic acid solvent in the presence of a catalyst consisting of a cobalt compound (e.g. bromide, hydroxide, etc.) and a bromine compound (e.g. Br, hydrogen bromide, etc.) at 130-150 deg.C. The amount of the acetic acid solvent is 0.8-3 times weight of m-nitrotoluene, that of the cobalt metal is 0.02-0.7wt% of acetic acid, and that of Br is 1-10 times, especially 2-5 times weight of the cobalt metal. A high quality objective compound can be obtained by this process, stably, with a small amount of catalyst at high reaction rate.

    PREPARATION OF M- OR P-NITROBENZOIC ACID

    公开(公告)号:JPS57185239A

    公开(公告)日:1982-11-15

    申请号:JP6764581

    申请日:1981-05-07

    Abstract: PURPOSE:To obtain the titled substance of high purity, by oxidizing m- or p- nitrotoluene in the absence of bromine in the presence of a Co compound as a catalyst and acetaldehyde as a promotor at a specific temperature and pressure in an inexpensive stainless steel apparatus. CONSTITUTION:In oxidizing p-nitrotoluene with molecular oxygen in acetic acid solvent to give the titled compound, a Co compound is used as a heavy metallic catalyst, and acetaldehyde is used as a promotor. The reaction is carried out in the absence of bromine at 110-140 deg.C and 3-30 atm. The amount of the acetic acid solvent is 1.5-6 times that of the nitrotoluene, and the Co compound, e.g. Co salt of a lower aliphatic carboxylic acid or cobalt carbonate, is used in an amount of 0.2-0.5wt% expressed in terms of metallic Co. The acetaldehyde is used in an amount of 0.5-1 based on the nitrotoluene. Preferably, the acetaldehyde is fed continuously and uniformly to the whole reactor. USE:A raw material for agricultural chemicals, medicines, and dyes.

    CONTINUOUS PREPARATION OF O-TOLUIC ACID

    公开(公告)号:JPS56156232A

    公开(公告)日:1981-12-02

    申请号:JP5865180

    申请日:1980-05-06

    Abstract: PURPOSE:To obtain o-toluic acid in the liquid phase continuously, by the oxidation of o-xylene with O2 in the presence of a Co catalyst at a specific temperature and pressure while controlling the amounts of a raw material to be supplied and the reaction product to be taken out to achieve the specific conversion. CONSTITUTION:o-Xylene is oxidized with molecular O2 gas in the liquid phase in the presence of a Co compound catalyst in an amount of 0.02-0.2wt% converted to Co, at 120-150 deg.C and 2-20atm, to give o-toluic acid continuously. The supplied amount of o-xylene and the gas containing molecular oxygen into the reactor and the amount of the reaction product to be taken out of a reactor are controlled so that the o-toluic acid contained in the reaction product has a concentration of 15-35wt% and the oxygen in the waste gas is 1-8vol%. EFFECT:This method may give the aimed high-purity compound and be economical.

    PURIFICATION OF TEREPHTHALIC ACID
    27.
    发明专利

    公开(公告)号:JPS5640639A

    公开(公告)日:1981-04-16

    申请号:JP11517379

    申请日:1979-09-10

    Abstract: PURPOSE:To obtain the purified terephthalic acid useful as a raw material for fibers by the specific treatment of impure terephthalic acid. CONSTITUTION:A solution of terephthalic acid containing an impurity to reduce the light transmittance at 340nm in an aqueous alkali is methylated by the addition of dimethylsulfuric acid in a molar amount of 0.1-1.0 time that of the terephthalic acid. The impurity has an unknown structure and comprises coloring substances. The terephthalic acid of low purity recovered from the purifying stage in the production of terephthalic acid or from the recovering stage of a solvent and a catalyst, may be purified readily.

    PREPARATION OF TEREPHTHALIC ACID
    28.
    发明专利

    公开(公告)号:JPS5476537A

    公开(公告)日:1979-06-19

    申请号:JP14077377

    申请日:1977-11-25

    Abstract: PURPOSE:To separate terephthalic acid, by oxidizing p-xylene in the liquid phase with air at a relatively low temperature, using paraldehyde or acetaldehyde, which will not contaminate the reaction system, as a reaction accelerator, followed by solid-liquid separation of the reaction product heat-treated at a somewhat higher temperature. CONSTITUTION:p-Xylene is oxidized in the liquid phase with a gas containing oxygen in the presence of a Co compound in acetic acid at 110-140 deg.C using paraldehyde or acetaldehyde as a reaction accelerator to give an oxidation product slurry, which is then kept at a temperature, preferably 140-170 deg.C, higher than the reaction temperature, and the terephthalic acid is separated from the slurry. The reaction accelerator may be used separately or in a mixture, and the amount is preferably 0.2-1 part by wt. pter part by wt. of p-xylene.

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